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4-Methylmorpholine → HCID 71533330、化合物

HRID 2173717
ノート
印刷プレビュー

反応式

HRID 2173717 の反応式
[NH2:1][C:2]1[C:3]([C:13]([OH:15])=O)=[N:4][C:5]([Br:12])=[C:6]([C:8]([F:11])([F:10])[F:9])[N:7]=1.[NH2:16][C:17]1[NH:21][N:20]=[CH:19][C:18]=1[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CN1CCOCC1>CN(C=O)C.O>[NH2:1][C:2]1[C:3]([C:13]([NH:16][C:17]2[NH:21][N:20]=[CH:19][C:18]=2[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=2)=[O:15])=[N:4][C:5]([Br:12])=[C:6]([C:8]([F:9])([F:10])[F:11])[N:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 79724-MethylmorpholineHCID 14777624-(2-Pyridinyl)-1H-pyrazol-3-amineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 584422963-Amino-6-bromo-5-trifluoromethyl-pyrazine-2-carboxylic acid2 回

生成物 1

HCID 71533330HCID 71533330、化合物

試薬・触媒・溶媒

2
HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture comprising 3-amino-6-bromo-5-trifluoromethyl-pyrazine-2-carboxylic acid (Intermediate 2) (0.179 g, 0.624 mmol), 5-amino-4-(pyridin-2-yl)-1H-pyrazole (0.1 g, 0.624 mmol), HATU (0.237 g, 0.624 mmol) and N-methylmorpholine (0.123 ml, 1.249 mmol) in DMF (5 ml) was stirred at 80° C. for 2.5 hours. After cooling to RT, the mixture was diluted with water (40 ml) and the resulting yellow precipitate was filtered under vacuum and washed with water (20 ml). MeOH (150 ml) was added to the solid and the suspension ultrasonicated to give a fine suspension. The suspension was filtered under vacuum and the solid was rinsed with MeOH (20 ml) and dried under vacuum at 45° C. for 1.5 hours to afford the title compound as a yellow solid.

後処理

  1. filtrationthe resulting yellow precipitate was filtered under vacuum
  2. washwashed with water (20 ml)
  3. additionMeOH (150 ml) was added to the solid
  4. customthe suspension ultrasonicated
  5. customto give a fine suspension
  6. filtrationThe suspension was filtered under vacuum
  7. washthe solid was rinsed with MeOH (20 ml)
  8. customdried under vacuum at 45° C. for 1.5 hours

出典と根拠

ORDレコード
ord-e5e86b7a72c84dabb34c2e4825ddab7e
出典データセット
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09056867B2

反応ノート

読み込み中…

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